CN106892411A - A kind of method for purifying selenium - Google Patents
A kind of method for purifying selenium Download PDFInfo
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- CN106892411A CN106892411A CN201710306227.2A CN201710306227A CN106892411A CN 106892411 A CN106892411 A CN 106892411A CN 201710306227 A CN201710306227 A CN 201710306227A CN 106892411 A CN106892411 A CN 106892411A
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- selenium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a kind of method for purifying selenium, comprises the following steps：1) with industrial selenium as raw material, in the atmosphere of CO, with N, N-dimethylformamide (DMF) is solvent, with inorganic base as cosolvent, in 0.1 0.6MPa, stirring reaction 10min at 10 50 DEG C, after completion of the reaction, take out solvent liquid, isolation air suction filtration, by the selenium solid lucifuge drying on funnel, obtains sulphur removal purifying selenium powder；2) sulphur removal purifying selenium powder is placed in CO atmosphere, with DMF as solvent, with organic base as cosolvent, in 0.1 0.4MPa, stirring reaction 20min at 25 50 DEG C, after completion of the reaction, takes out solvent liquid, isolation air suction filtration, takes solid, washing, lucifuge drying, obtains pure selenium powder.The present invention is easy to operate and safe, and is reacted under normal temperature and pressure, and reaction condition is gentle.
Description
Technical field
The present invention relates to selenium purification field, and in particular to a kind of method of purification selenium.
Background technology
Selenium as important rare dissipated metal material oneself be widely used in electronics industry, metallurgical industry, glass industry,
Chemical color industry, biological field, cosmetics industry, agricultural, medicines and health protection food industry etc., and these industries are to the purity of selenium
It is less demanding.But with the development of science and technology, purity requirement of the high-tech industry to selenium is high, such as semiconductor equipment, photoelectricity equipment,
The manufacture of Se solar cell, laser device, laser and infrared ray optical direction material etc..Conventionally produced selenium purity can only achieve
99.99% or so, it is impossible to meet the requirement of high-precision end industry, the removing of wherein impurity S, Te, AL, Pd, Hg, As, Fe etc. is system
Take the biggest problem that high-purity selenium faces.At present, high-purity selenium method of purification mainly has impure selenium voloxidation method, vacuum distillation method, area
Domain smelting process and H2Se thermal decomposition methods etc..Mainly there are Germany, Japan, Chile etc. in the country of foreign countries' production high-purity selenium, but external
Company all employs strict secrecy technology to the key technology of high-purity selenium purifying technique, is difficult to look in the document published
To relevant report.Domestic high-purity selenium purifying technique and analysis means and developed country have certain gap for comparing, and purify
The technique of selenium is mostly using oxidizing process and adsorption precipitation, neutralizing hydrolysis method joint purification selenium, or prime ion-exchange, rear class
Carry out purifying etc. the method for purification of traditional selenium with solvent extraction, these methods have that technological process is long, seriously polluted, reclaim
The shortcoming that rate is low, high cost and large-scale production are difficult.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of method for purifying selenium, with industrial selenium as raw material, in CO atmosphere
Under, in organic solvent DMF, using sodium acetate and DBU for cosolvent is processed successively, impure selenium is purified under normal temperature and pressure, its operation letter
Just it is, with low cost.
The technical solution adopted by the present invention is：
A kind of method for purifying selenium, comprises the following steps：
1) with industrial selenium as raw material, in the atmosphere of CO, with N, N-dimethylformamide (DMF) is solvent, with inorganic base
It is cosolvent, in 0.1-0.6MPa, stirring reaction 10min at 10-50 DEG C after completion of the reaction, takes out solvent liquid, completely cuts off air
Suction filtration, by the selenium solid lucifuge drying on funnel, obtains sulphur removal purifying selenium powder；
2) sulphur removal purifying selenium powder is placed in CO atmosphere, with DMF as solvent, with organic base as cosolvent, 0.1-
0.4MPa, stirring reaction 20min at 25-50 DEG C, after completion of the reaction, take out solvent liquid, completely cut off air suction filtration, take solid, wash
Wash, lucifuge is dried, and obtains pure selenium powder.
A kind of method of described purification selenium, step 1) in inorganic base be sodium acetate.
A kind of method of described purification selenium, step 1) in the matter liquor ratio of sodium acetate and DMF be 1:20, g/L.
A kind of method of described purification selenium, repeat step 1) 2-4 times industrial selenium is processed, obtain sulphur removal purifying selenium
Powder.
A kind of method of described purification selenium, step 2) in organic base for the carbon of 1,8- diazabicylos [5.4.0] 11-
7- alkene (DBU).
A kind of method of described purification selenium, step 2) in the carbon -7- alkene volume of 1,8- diazabicylos [5.4.0] 11 use
Measure is the 0.5% of DMF volumes.
A kind of method of described purification selenium, repeat step 2) 2-4 times to sulphur removal purifying selenium powder process, obtain pure selenium
Powder.
A kind of method of described purification selenium, step 2) in take out solvent liquid after completion of the reaction, completely cut off air suction filtration, filtrate
Refiltered after stirring 30min in atmosphere, take solid and through 3-5 washing, lucifuge drying obtains pure selenium powder.
The invention has the advantages that：
A kind of method for purifying selenium of the present invention is as raw material, according to impurity such as selenium and sulphur, telluriums with industrial impure selenium (about 98%)
Behavior difference at different conditions, with N, N-dimethylformamide (DMF) is solvent, in the closing of uniform temperature and pressure
In system, cosolvent is first done except the sulphur impurity in impure selenium with inorganic base sodium acetate；Then again with 1,8-diazabicylo of organic base
11 carbon-7-alkene (DBU) are cosolvent except impurity such as the telluriums in impure selenium so that impure selenium can be purified preferably.This hair
It is bright easy to operate and safe, and reacted under normal temperature and pressure, reaction condition is gentle.
The present invention is not harsh to temperature and pressure requirement, and reaction dissolvent can be recycled, and equipment investment is few, simple to operate
It is convenient.
DMF is used as reaction dissolvent for the present invention, cheap and easy to get, and stirs and easily separated with product (solid-liquid point after reaction
From).
The present invention is with a small amount of inorganic base sodium acetate as cosolvent.With a small amount of organic base DBU as cosolvent.
The present invention is environmentally friendly, will not produce toxic gas, to operating personnel almost without health threat.
Good economy performance of the present invention, can improve impure selenium purity using reaction purification.
Specific embodiment
Following is that, to detailed description of the invention, raw material is industrial impure selenium, and wherein Se content is 98.13%.
A kind of method for purifying selenium of embodiment one
Comprise the following steps：
1) this step mainly removes sulphur impurity：The addition 1kg industry impure selenium powder in the 200L reactors equipped with agitator, then to
It adds 5g sodium acetates, is subsequently adding 100L DMF, with vacuum pumped air, is passed through CO and takes a breath four times, 0.1-
10min is reacted at 0.6MPa, 10-50 DEG C, reaction is finished, take out solvent liquid, completely cut off air suction filtration, the selenium solid on funnel is kept away
Light is dried, and obtains sulphur removal purifying selenium powder.
Repeat step 1) industrial impure selenium powder is processed for three times, it is per treatment after obtain sulphur removal purifying selenium powder and examined
Survey, testing result is as shown in table 1.
Table 1 is each step 1) treatment after sulphur removal purifying selenium powder in sulphur content.
| Element | Raw material | Single treatment | After-treatment | Three treatment |
| S | 0.30% | 0.17% | 0.12% | 0.09% |
2) this step is except impurity such as Te, AL, Pd, As, Fe：Added through step 1 in the 200L reactors equipped with agitator)
1kg sulphur removal purifying selenium powder after single treatment, then adds 0.5L DBU to it, is subsequently adding 100L DMF, uses vacuum pumping
Go out air, be passed through CO and take a breath four times, in 0.1-0.4MPa, 20min is reacted at 25-50 DEG C, reaction is finished, and takes out solvent liquid,
Isolation air suction filtration, filtrate refilters after stirring 30min in atmosphere, takes solid and repeatedly wash, lucifuge drying, obtains pure selenium
Powder.
Repeat step 2) three times to step 1) the sulphur removal purifying selenium powder after single treatment reprocesses, every time by step
2) obtain pure selenium powder after processing and detected that testing result is as shown in table 2.
Table 2 is each step 2) content of impurity in pure selenium powder is obtained after treatment.
| Element | Raw material | Single treatment | After-treatment | Three treatment |
| Te | 0.980% | 0.517% | 0.331% | 0.105% |
| Al | 0.143% | 0.095% | 0.068% | 0.022% |
| As | 0.087% | 0.052% | 0.034% | 0.011% |
| B | 0.020% | 0.011% | 0.007% | 0.003% |
| Bi | 0.037% | 0.017% | 0.005% | 0.002% |
| Cu | 0.132% | 0.047% | 0.008% | 0.001% |
| Fe | 0.154% | 0.038% | 0.010% | 0.002% |
| Ga | 0.006% | 0.003% | 0.002% | 0.002% |
| Li | 0.031% | 0.021% | 0.013% | 0.004% |
| Mg | 0.023% | 0.010% | 0.003% | 0.002% |
| Pb | 0.108% | 0.063% | 0.027% | 0.009% |
| Sb | 0.041% | 0.018% | 0.006% | 0.002% |
| Ti | 0.034% | 0.024% | 0.011% | 0.003% |
| Tl | 0.056% | 0.032% | 0.019% | 0.001% |
| V | 0.012% | 0.008% | 0.007% | 0.007% |
Claims (8)
1. it is a kind of purify selenium method, it is characterised in that comprise the following steps：
1) with industrial selenium as raw material, in the atmosphere of CO, with N, N-dimethylformamide (DMF) is solvent, with inorganic base to help
Solvent, in 0.1-0.6MPa, stirring reaction 10min at 10-50 DEG C after completion of the reaction, takes out solvent liquid, completely cuts off air suction filtration,
By the selenium solid lucifuge drying on funnel, sulphur removal purifying selenium powder is obtained；
2) sulphur removal purifying selenium powder is placed in CO atmosphere, with DMF as solvent, with organic base as cosolvent, in 0.1-0.4MPa,
Stirring reaction 20min at 25-50 DEG C, after completion of the reaction, takes out solvent liquid, completely cuts off air suction filtration, takes solid, washing, lucifuge baking
It is dry, obtain pure selenium powder.
2. a kind of method for purifying selenium as claimed in claim 1, it is characterised in that step 1) in inorganic base be sodium acetate.
3. a kind of method for purifying selenium as claimed in claim 2, it is characterised in that step 1) in sodium acetate and DMF matter liquid
Than being 1:20, g/L.
4. a kind of method for purifying selenium as claimed in claim 1, it is characterised in that repeat step 1) 2-4 times industrial selenium is entered
Row treatment, obtains sulphur removal purifying selenium powder.
5. a kind of method for purifying selenium as claimed in claim 1, it is characterised in that step 2) in organic base be 1,8- phenodiazines
Carbon -7- alkene (DBU) of miscellaneous two ring [5.4.0] 11.
6. a kind of method for purifying selenium as claimed in claim 5, it is characterised in that step 2) in 1,8- diazabicylos
[5.4.0] 11 carbon -7- alkene volumetric usage is the 0.5% of DMF volumes.
7. a kind of method for purifying selenium as claimed in claim 1, it is characterised in that repeat step 2) 2-4 time to sulphur removal purifying
Selenium powder is processed, and obtains pure selenium powder.
8. a kind of method for purifying selenium as claimed in claim 1, it is characterised in that step 2) in take out solvent after completion of the reaction
Liquid, completely cuts off air suction filtration, and filtrate refilters after stirring 30min in atmosphere, takes solid and through 3-5 washing, and lucifuge is dried,
Obtain pure selenium powder.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710306227.2A CN106892411B (en) | 2017-05-04 | 2017-05-04 | A method of purification selenium |
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| CN201710306227.2A CN106892411B (en) | 2017-05-04 | 2017-05-04 | A method of purification selenium |
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| CN106892411A true CN106892411A (en) | 2017-06-27 |
| CN106892411B CN106892411B (en) | 2018-09-21 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6217007A (en) * | 1985-07-12 | 1987-01-26 | Mitsubishi Metal Corp | Method for recovering or purifying selenium |
| CN102086029A (en) * | 2010-12-04 | 2011-06-08 | 金川集团有限公司 | Method for extracting selenium from selenium-contained material |
| CN103328379A (en) * | 2011-04-18 | 2013-09-25 | 昭和电工株式会社 | Process for producing carbonyl sulfide |
-
2017
- 2017-05-04 CN CN201710306227.2A patent/CN106892411B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6217007A (en) * | 1985-07-12 | 1987-01-26 | Mitsubishi Metal Corp | Method for recovering or purifying selenium |
| CN102086029A (en) * | 2010-12-04 | 2011-06-08 | 金川集团有限公司 | Method for extracting selenium from selenium-contained material |
| CN103328379A (en) * | 2011-04-18 | 2013-09-25 | 昭和电工株式会社 | Process for producing carbonyl sulfide |
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| CN106892411B (en) | 2018-09-21 |
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